US11399560B2 - Capsules containing two phases and method for their preparation - Google Patents

Capsules containing two phases and method for their preparation Download PDF

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Publication number
US11399560B2
US11399560B2 US15/577,296 US201615577296A US11399560B2 US 11399560 B2 US11399560 B2 US 11399560B2 US 201615577296 A US201615577296 A US 201615577296A US 11399560 B2 US11399560 B2 US 11399560B2
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Prior art keywords
calcium
alginate
solution
phases
ions
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US20180146704A1 (en
Inventor
Ramon Ramon Real
Ramon Maria RAMON FERRES
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Caviaroli SL
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Caviaroli SL
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Assigned to CAVIAROLI, S.L. reassignment CAVIAROLI, S.L. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: RAMON FERRES, Ramon Maria, RAMON REAL, RAMON
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Classifications

    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00Shaping or working of foodstuffs characterised by the products
    • A23P10/30Encapsulation of particles, e.g. foodstuff additives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings or cooking oils
    • A23D9/007Other edible oils or fats, e.g. shortenings or cooking oils characterised by ingredients other than fatty acid triglycerides
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23DEDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
    • A23D9/00Other edible oils or fats, e.g. shortenings or cooking oils
    • A23D9/02Other edible oils or fats, e.g. shortenings or cooking oils characterised by the production or working-up
    • A23D9/04Working-up
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23GCOCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G1/00Cocoa; Cocoa products, e.g. chocolate; Substitutes therefor
    • A23G1/30Cocoa products, e.g. chocolate; Substitutes therefor
    • A23G1/50Cocoa products, e.g. chocolate; Substitutes therefor characterised by shape, structure or physical form, e.g. products with an inedible support
    • A23G1/54Composite products, e.g. layered, laminated, coated or filled
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23GCOCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
    • A23G3/00Sweetmeats; Confectionery; Marzipan; Coated or filled products
    • A23G3/34Sweetmeats, confectionery or marzipan; Processes for the preparation thereof
    • A23G3/50Sweetmeats, confectionery or marzipan; Processes for the preparation thereof characterised by shape, structure or physical form, e.g. products with supported structure
    • A23G3/54Composite products, e.g. layered, coated, filled
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/50Soya sauce
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/60Salad dressings; Mayonnaise; Ketchup
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/70Fixation, conservation, or encapsulation of flavouring agents
    • A23L27/72Encapsulation
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A23L29/206Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin
    • A23L29/256Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents of vegetable origin from seaweeds, e.g. alginates, agar or carrageenan
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23PSHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P20/00Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
    • A23P20/10Coating with edible coatings, e.g. with oils or fats
    • A23P20/105Coating with compositions containing vegetable or microbial fermentation gums, e.g. cellulose or derivatives; Coating with edible polymers, e.g. polyvinyalcohol
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • A61K9/16Agglomerates; Granulates; Microbeadlets ; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction
    • A61K9/1682Processes

Definitions

  • the present invention refers to capsules coated with a calcium alginate film which contain two mutually immiscible or partly miscible phases, such as an aqueous phase and a hydrophobic phase or a liquid phase and a solid phase, for example. Moreover, the present invention also refers to the method by which said two phases can be encapsulated and kept stable within the formed capsule.
  • the inventor of the present invention is not aware of the existence of capsules coated with calcium alginate which have two mutually immiscible or partly miscible phases in the interior thereof.
  • the biphasic capsules of the present invention can be obtained by a method usually known as “spherification”, either by direct or reverse spherification.
  • the substance to be encapsulated and a non-calcium alginate are pumped through two concentric tubes with flow volumes that allow a drop of the substance to be encapsulated to be formed covered by a film of non-calcium alginate solution, which acts as a gelling agent. It is also possible to mix the alginate with the substance to be encapsulated. Said drop falls into a bath containing a source of calcium ions, forming a layer of gel which contains the material to be encapsulated. Said film is formed almost instantaneously on the outside and is semi-solid and gelatinous, while holding the encapsulated substance inside, in solid form if the calcium ions can migrate and in liquid form if the calcium ions cannot migrate.
  • the substance to be encapsulated is mixed with a source of calcium ions or magnesium ions, for example calcium chloride or other calcium salt.
  • a drop or other shape is formed with said mixture of the substance to be encapsulated and calcium ions or magnesium ions, and is introduced in a solution containing a non-calcium alginate, such as sodium alginate, for example.
  • a semi-solid, calcium alginate gelatinous film forms almost instantaneously, which holds within it the substance to be encapsulated.
  • the inventor of the present invention has developed a spherification method by which capsules containing two substances which form two mutually immiscible or partly miscible phases can be obtained on an industrial scale, and which surprisingly are spherical shaped and, in addition, it is possible for the diameter of said capsules to be up to 50 mm without affecting the sphericity thereof, preferably within a range from 5 mm to 50 mm, more preferably from 10 mm to 50 mm, yet more preferably from 15 mm to 50 mm, from 20 mm to 50 mm, from 25 mm to 50 mm and most preferably from 30 mm to 50 mm.
  • the method according to the present invention is based on the use of two concentric tubes which form the two-phase drop to be encapsulated and the gelling solution, it being necessary that the substance applied through the outer tube should comprise a source of calcium ions or magnesium ions.
  • the production of the biphasic capsules takes place using a method known as reverse spherification with some variations.
  • the present invention therefore discloses a method for producing capsules of biphasic substances, characterised in that it comprises the following steps:
  • the method of the present invention can be used both in the food industry and in the cosmetic, intraceutical, chemical or pharmaceutical industries, or any other industry that requires this type of capsule.
  • the method of the present invention allows biphasic spheres to be obtained but clearly a person skilled in the art would be able to carry out said two-phase sphere encapsulation by other known methods, such as direct spherification or other variants of reverse spherification.
  • biphasic substances are understood to be two substances that are mutually immiscible or partly miscible. They may be organic or inorganic substances provided they comply with the above.
  • biphasic is understood in the present document to refer to two phases that are mutually immiscible or partly miscible, and may contain both two liquid phases, a liquid-solid phase where the solid can be obtained with or without a reaction, a liquid-gas phase, and in addition a person skilled in the art could use additives to emulsify the encapsulated solutions and obtain biphasic spheres that are more stable over time.
  • biphasic spheres obtained by freezing one of the two phases and a subsequent direct or reverse spherification reaction, by means of a method known as frozen spherification are also within the scope of the present invention.
  • a sphere of oil obtained by direct spherification can be included in a solution of vinegar with a source of calcium, which after contact with the alginate creates a sphere surrounded by a film of alginate which has within it said sphere of oil. It may also include a solid phase of a frozen or gelled product which is incorporated in said calcium-rich solution for subsequent gelling.
  • liquid paraffins or paraffin waxes, petroleum jellies, plant oils, waxes, fatty alcohols and their esters, lanolin and silicon and mixtures thereof can be used as the oleous phase.
  • biphasic spheres can be obtained such as vinegar-oil, soy sauce-sesame oil, mustard-olive oil, honey-olive oil and coffee-chocolate, among others.
  • vinegar-oil soy sauce-sesame oil
  • mustard-olive oil mustard-olive oil
  • honey-olive oil honey-olive oil
  • coffee-chocolate among others.
  • a person skilled in the art will understand that any combination of substances that form two mutually immiscible or partly miscible phases can be used for encapsulation according to the method of the present invention.
  • said mutually immiscible or partly miscible substances can be mixed with seasonings, perfumes, flavourings and other oil-soluble additives.
  • the aqueous solution containing calcium ions used in the method of the present invention could be any source of calcium ions, provided it can form a calcium alginate gel which forms the outer film of the capsule.
  • sources of calcium ions can be mentioned calcium chloride, calcium lactate, calcium gluconate, for example, or a mixture thereof.
  • the source of calcium ions is calcium chloride.
  • said solution of calcium ions may contain any type of additive or may be mixed with any raw material that allows the organoleptic characteristics of the capsule obtained to be modified.
  • the alginate solution of the method of the present invention may be any non-calcium alginate salt, provided it reacts in the presence of calcium ions and forms the outer film of calcium alginate of the capsules.
  • the alginate used is sodium alginate.
  • the pH of the alginate solution is between 2 and 14.
  • An additional advantage of the method of the present invention is that all the steps are carried out at ambient temperature.
  • An increase or reduction in temperature, as well as increasing the production cost of the capsules, may affect the viscosity, density and surface tension of the oleous and aqueous phases present in the method, and it would therefore be necessary to modify various process parameters to obtain the same results as at ambient temperature.
  • Drops were produced through two concentric tubes, and said drops containing olive oil in the inside tube and the prepared vinegar solution in the outer tube were introduced into a bath of the sodium alginate solution at ambient temperature. Said drops were collected and placed in a bath of water for washing. They were drained and packed. At least one capsule 45 mm in diameter was obtained, which contained two phases of olive oil and vinegar.
  • Drops were produced through two concentric tubes, and said drops containing sesame oil in the inside tube and the prepared soy sauce solution in the outer tube were introduced into a bath of the sodium alginate solution at ambient temperature. Said drops were collected and placed in a bath of water for washing. They were drained and packed. Capsules 22 mm in diameter were obtained, which contained two phases of sesame oil and soy sauce.
  • Drops were produced through two concentric tubes, and said drops containing jojoba oil and vitamin E in the inside tube and the prepared caffeine solution in the outer tube were introduced into a bath of the sodium alginate solution at ambient temperature. Said drops were collected and placed in a bath of water for washing. They were drained and packed. At least one capsule 16 mm in diameter was obtained, which contained two phases of jojoba oil with vitamin E and caffeine.
  • a solution containing coffee and 1% by weight of xanthan gum was prepared and 0.2% by weight of calcium chloride was added.
  • Liquid chocolate was also prepared and sodium alginate 0.2% by weight was added.
  • Drops were produced through two concentric tubes, and said drops containing the liquid chocolate solution in the inside tube and the prepared coffee solution in the outer tube were introduced into a bath of the 0.3% sodium alginate solution at ambient temperature.
  • the outer layer of the coffee solution reacted with the alginate forming a film of calcium alginate on the outside.
  • the calcium included in the coffee reacted with the sodium alginate included in the chocolate, forming an outer film on the chocolate.
  • This chocolate solidified completely, and at least one capsule 10 mm in diameter was obtained, which contained two phases: a solid chocolate phase and a liquid coffee phase.
  • Drops were produced through two concentric tubes, and said drops containing olive oil macerated with rosemary in the inside tube and the prepared vinegar solution in the outer tube were introduced into a bath of 0.3% sodium alginate solution at ambient temperature. Said drops were collected and placed in a bath of water for washing. They were drained and packed. At least one capsule 28 mm in diameter was obtained, which contained two phases of olive oil macerated with rosemary and vinegar.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Dispersion Chemistry (AREA)
  • Biotechnology (AREA)
  • General Health & Medical Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • Medicinal Chemistry (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • General Preparation And Processing Of Foods (AREA)
  • Cosmetics (AREA)
  • Formation And Processing Of Food Products (AREA)
  • Medicinal Preparation (AREA)
US15/577,296 2015-05-27 2016-03-14 Capsules containing two phases and method for their preparation Active 2037-03-03 US11399560B2 (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
ES201530738A ES2541504B1 (es) 2015-05-27 2015-05-27 Cápsulas que contienen dos fases y procedimiento de obtención de las mismas
ESES201530738 2015-05-27
ESP201530738 2015-05-27
PCT/ES2016/070160 WO2016189171A1 (fr) 2015-05-27 2016-03-14 Capsules contenant deux phases et procédé pour les préparer

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US20180146704A1 US20180146704A1 (en) 2018-05-31
US11399560B2 true US11399560B2 (en) 2022-08-02

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EP (1) EP3305084B1 (fr)
JP (1) JP6689963B2 (fr)
ES (1) ES2541504B1 (fr)
PT (1) PT3305084T (fr)
WO (1) WO2016189171A1 (fr)

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DE202018000041U1 (de) * 2018-01-05 2018-02-23 Ulrich Brunner Sphärisches Produkt
US20190328019A1 (en) * 2018-04-26 2019-10-31 Stephanie Ann Green Olive Oil Pods or O2 Pods
ES2910373T3 (es) * 2018-05-18 2022-05-12 Unilever Ip Holdings B V Composición alimenticia emulsionada
EP3849342A1 (fr) * 2018-09-12 2021-07-21 CDJ Partners, LLC Sphères comestibles contenant de l'alcool
BR112021006627A2 (pt) * 2018-10-29 2021-07-06 Procter & Gamble composição líquida encapsulada
US12145120B2 (en) 2019-02-21 2024-11-19 Sushanta MITRA Liquid encapsulation method and compositions and uses related thereto
CN110200075B (zh) * 2019-07-18 2021-07-09 江南大学 一种茶乳风味双层爆珠及其制备方法
IT202100006698A1 (it) * 2021-03-19 2022-09-19 Univ Degli Studi Di Sassari Metodo per realizzare una sfera edibile contenente una matrice liquida
JP7281116B2 (ja) * 2021-05-11 2023-05-25 大日本印刷株式会社 乾燥マイクロキャリアおよびその製造方法
ES1284889Y (es) 2021-10-04 2022-04-04 Caviaroli S L Capsula coloreada con pigmentos

Citations (8)

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GB762700A (en) 1954-05-17 1956-12-05 Alginate Ind Ltd Improvements in or relating to encapsulation
EP0116311A1 (fr) 1983-01-17 1984-08-22 Morishita Jintan Co., Ltd. Capsules molles doubles et leur production
US4702921A (en) 1984-07-11 1987-10-27 Q.P. Corporation Method for preparing fish-egg-like edible products
WO2009022909A1 (fr) * 2007-08-16 2009-02-19 Friesland Brands B.V. Liquides comestibles encapsulés
US20090291168A1 (en) * 2001-12-24 2009-11-26 Thomas Mangos Mononuclearly filled microcapsules
EP2289494A1 (fr) 2002-04-04 2011-03-02 FMC Biopolymer AS Capsules de polysaccharide et procédés de préparation
GB2480361A (en) 2010-05-14 2011-11-16 Inst Chemii Fizycznej Polskiej Akademii Nauk Core shell capsules
GB2486945A (en) * 2010-12-14 2012-07-04 Inst Chemii Fizycznej Polskiej Akademii Nauk Method for producing capsules

Patent Citations (8)

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Publication number Priority date Publication date Assignee Title
GB762700A (en) 1954-05-17 1956-12-05 Alginate Ind Ltd Improvements in or relating to encapsulation
EP0116311A1 (fr) 1983-01-17 1984-08-22 Morishita Jintan Co., Ltd. Capsules molles doubles et leur production
US4702921A (en) 1984-07-11 1987-10-27 Q.P. Corporation Method for preparing fish-egg-like edible products
US20090291168A1 (en) * 2001-12-24 2009-11-26 Thomas Mangos Mononuclearly filled microcapsules
EP2289494A1 (fr) 2002-04-04 2011-03-02 FMC Biopolymer AS Capsules de polysaccharide et procédés de préparation
WO2009022909A1 (fr) * 2007-08-16 2009-02-19 Friesland Brands B.V. Liquides comestibles encapsulés
GB2480361A (en) 2010-05-14 2011-11-16 Inst Chemii Fizycznej Polskiej Akademii Nauk Core shell capsules
GB2486945A (en) * 2010-12-14 2012-07-04 Inst Chemii Fizycznej Polskiej Akademii Nauk Method for producing capsules

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"Reverse Spherification"—Adventures in Molecular Cooking [2]; Accessible on the World Wide Web at https://mylastbite.wordpress.com/2008/12/22/adventures-in-molecular-cooking-2/; Dec. 22, 2008.
ANILKUMAR G. GAONKAR, NIRAJ VASISHT, ATUL RAMESH KHARE, ROBERT SOBEL (EDS.): "Microencapsulation in the Food Industry: A Practical Implementation Guide", 1 August 2014, ELSEVIER SCIENCE ELSEVIER SCIENCE , US , ISBN: 978-0-12-404735-8, article THORSTEN BRANDAU: "Chapter 10: Annular Jet-Based Processes", pages: 99 - 110, XP055271852, DOI: 10.1016/B978-0-12-404568-2.00010-8
Brandau Microencapsulation in the Food Industry, Chapter 10, 2014 ,p. 109. *
Brandau, T., Chapter 10: Annular Jet-Based Processes, Microencapsulation in the Food Industry: A Practical Implementation Guide, Elsevier Science, XP055271852, ISBN: 978-0-12-404735-8, pp. 99-110, Aug. 1, 2014.
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Also Published As

Publication number Publication date
JP6689963B2 (ja) 2020-04-28
EP3305084B1 (fr) 2024-02-14
PT3305084T (pt) 2024-03-14
ES2541504A1 (es) 2015-07-20
HK1253285A1 (en) 2019-06-14
US20180146704A1 (en) 2018-05-31
EP3305084A1 (fr) 2018-04-11
WO2016189171A1 (fr) 2016-12-01
JP2018516598A (ja) 2018-06-28
ES2541504B1 (es) 2016-02-01

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